関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 反応物 | (2R)-1-(benzyloxy)pent-4-en-2-ol | HCID 10375318 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [(R)-2-(2,2-diethoxyethoxy)-4-pentenyloxymethyl]benzene | HCID 59281174 | — |
反応手順
(R)-1-Benzyloxy-4-penten-2-ol (3.13 g) was dissolved in DMF (32 ml), and sodium hydride (60%, 0.91 g) was added in an ice bath. After stirring at the same temperature for 30 minutes, bromoacetaldehyde diethyl acetal (3.03 ml) was added. The mixture was heated to room temperature and stirred for two hours, and then heated to 50° C. and stirred for one hour. After cooling to room temperature, ice was added to the reaction solution. The reaction solution was extracted with ethyl acetate. The organic layer was washed with water and brine. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound. The mixture containing the recovered raw material was reacted under the same conditions. The title compound was obtained by purification by the same method (total yield: 5.00 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08198269B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-3667462c2a6245cf8e89e8e792959184 |
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| 出典メモ | uspto-grants-2012_06 |
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